+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2005src1567 started at 13:47:36 on 01-Dec-2005 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2005src1567 in I-4 CELL 0.71073 16.8137 16.8137 13.9960 90.000 90.000 90.000 ZERR 8.00 0.0004 0.0004 0.0005 0.000 0.000 0.000 LATT -2 SYMM - X, - Y, Z SYMM Y, - X, - Z SYMM - Y, X, - Z SFAC C H O UNIT 168 272 8 V = 3956.68 F(000) = 1344.0 Mu = 0.06 mm-1 Cell Wt = 2419.86 Rho = 1.016 MERG 4 OMIT -3.00 55.00 OMIT 1 4 1 OMIT 0 0 2 OMIT 0 3 3 OMIT 1 1 2 OMIT -2 4 0 OMIT -1 5 0 OMIT 2 2 2 SADI C6 C7 C6 C27 SHEL 7 0.77 EQIV $1 -Y, X, -Z HTAB O1 O1_$1 FMAP 2 PLAN 5 SIZE 0.09 0.16 0.32 ACTA BOND $H WGHT 0.04600 1.56480 L.S. 8 TEMP -153.00 FVAR 0.63098 0.63851 C1 1 0.375031 -0.010481 -0.037839 11.00000 0.06434 0.05812 = 0.07518 -0.02866 -0.02726 0.03057 AFIX 93 H1A 2 0.405406 0.015126 -0.086103 11.00000 -1.20000 H1B 2 0.373730 -0.066898 -0.034489 11.00000 -1.20000 AFIX 0 C2 1 0.334865 0.032087 0.024215 11.00000 0.03605 0.03569 = 0.05606 -0.01170 -0.01158 0.00692 AFIX 43 H2 2 0.305446 0.003671 0.071044 11.00000 -1.20000 AFIX 0 C3 1 0.330782 0.121141 0.028561 11.00000 0.02793 0.03330 = 0.03079 -0.00174 0.00106 0.00284 AFIX 13 H3 2 0.353105 0.141856 -0.032811 11.00000 -1.20000 AFIX 0 C4 1 0.241896 0.147785 0.033283 11.00000 0.02515 0.02925 = 0.02950 -0.00043 0.00199 0.00230 AFIX 13 H4 2 0.215658 0.110735 0.079439 11.00000 -1.20000 AFIX 0 C5 1 0.201159 0.132618 -0.063998 11.00000 0.03175 0.04398 = 0.03302 -0.00588 -0.00022 0.00524 AFIX 23 H5A 2 0.224643 0.169029 -0.111895 11.00000 -1.20000 H5B 2 0.213228 0.077550 -0.084413 11.00000 -1.20000 AFIX 0 C6 1 0.111393 0.143756 -0.064301 11.00000 0.03036 0.05237 = 0.03373 -0.00302 -0.00273 0.00453 AFIX 13 H6 2 0.101845 0.195053 -0.030009 11.00000 -1.20000 AFIX 0 PART 1 C7 1 0.076746 0.155810 -0.164489 21.00000 0.03382 0.03244 = 0.03702 0.00338 -0.00547 -0.00385 AFIX 23 H7A 2 0.018946 0.166063 -0.158986 21.00000 -1.20000 H7B 2 0.101553 0.203335 -0.193741 21.00000 -1.20000 AFIX 0 C8 1 0.089736 0.084962 -0.229581 21.00000 0.03677 0.04632 = 0.04245 -0.00624 -0.00302 -0.00026 AFIX 23 H8A 2 0.069316 0.036396 -0.197996 21.00000 -1.20000 H8B 2 0.147468 0.077764 -0.240468 21.00000 -1.20000 AFIX 0 C9 1 0.048161 0.095531 -0.325132 21.00000 0.04737 0.06522 = 0.04562 -0.00921 -0.00451 -0.00648 AFIX 137 H9A 2 -0.009347 0.099671 -0.314878 21.00000 -1.50000 H9B 2 0.059487 0.049633 -0.366089 21.00000 -1.50000 H9C 2 0.067529 0.144105 -0.356058 21.00000 -1.50000 AFIX 0 PART 2 SAME C7 > C9 C27 1 0.071825 0.105625 -0.159562 -21.00000 0.03230 0.03019 = 0.03847 0.00491 -0.00043 -0.00359 AFIX 23 H27A 2 0.096304 0.053377 -0.173668 -21.00000 -1.20000 H27B 2 0.014023 0.097745 -0.149975 -21.00000 -1.20000 AFIX 0 C28 1 0.086236 0.162750 -0.241716 -21.00000 0.04422 0.03910 = 0.03841 -0.00348 -0.00438 -0.00649 AFIX 23 H28A 2 0.144096 0.167750 -0.253378 -21.00000 -1.20000 H28B 2 0.065335 0.215988 -0.224910 -21.00000 -1.20000 AFIX 0 C29 1 0.044903 0.132491 -0.332753 -21.00000 0.05383 0.05887 = 0.02862 -0.00058 -0.01116 -0.01145 AFIX 137 H29A 2 0.067730 0.081116 -0.351238 -21.00000 -1.50000 H29B 2 0.052772 0.170937 -0.384524 -21.00000 -1.50000 H29C 2 -0.012132 0.126138 -0.320506 -21.00000 -1.50000 AFIX 0 PART 0 C10 1 0.383396 0.153879 0.110139 11.00000 0.03141 0.02850 = 0.03561 -0.00026 -0.00375 0.00177 AFIX 13 H10 2 0.373355 0.212387 0.114533 11.00000 -1.20000 AFIX 0 C11 1 0.471749 0.142534 0.086268 11.00000 0.02953 0.06159 = 0.04404 0.00279 -0.00349 -0.00304 AFIX 137 H11A 2 0.504318 0.168792 0.135022 11.00000 -1.50000 H11B 2 0.483095 0.165948 0.023611 11.00000 -1.50000 H11C 2 0.484259 0.085618 0.084925 11.00000 -1.50000 AFIX 0 C12 1 0.364766 0.118245 0.206999 11.00000 0.03937 0.05665 = 0.03713 0.00531 -0.00233 0.00331 AFIX 137 H12A 2 0.376088 0.061077 0.205870 11.00000 -1.50000 H12B 2 0.308453 0.126697 0.221937 11.00000 -1.50000 H12C 2 0.397706 0.143909 0.255850 11.00000 -1.50000 AFIX 0 C13 1 0.227760 0.231535 0.072829 11.00000 0.02405 0.03278 = 0.02761 -0.00017 -0.00187 0.00307 C14 1 0.261782 0.300305 0.032328 11.00000 0.03094 0.03612 = 0.03446 0.00577 0.00225 0.00466 C15 1 0.248143 0.374029 0.073989 11.00000 0.03188 0.02832 = 0.04176 0.00737 -0.00125 0.00051 AFIX 43 H15 2 0.271570 0.419759 0.045755 11.00000 -1.20000 AFIX 0 C16 1 0.201949 0.383614 0.154738 11.00000 0.03164 0.03051 = 0.03782 -0.00493 -0.01189 0.00358 C17 1 0.168053 0.316032 0.193709 11.00000 0.02425 0.03639 = 0.02855 -0.00525 -0.00272 0.00256 AFIX 43 H17 2 0.136127 0.321051 0.249385 11.00000 -1.20000 AFIX 0 C18 1 0.179169 0.240860 0.154043 11.00000 0.02293 0.03202 = 0.02920 -0.00250 -0.00418 0.00025 C19 1 0.314744 0.299595 -0.055185 11.00000 0.05869 0.03956 = 0.04843 0.01349 0.01828 0.00562 AFIX 137 H19A 2 0.325667 0.354385 -0.075143 11.00000 -1.50000 H19B 2 0.287928 0.271162 -0.107130 11.00000 -1.50000 H19C 2 0.364909 0.272779 -0.039914 11.00000 -1.50000 AFIX 0 C20 1 0.186518 0.464720 0.197240 11.00000 0.05002 0.03401 = 0.05430 -0.00883 -0.00959 0.00398 AFIX 137 H20A 2 0.217426 0.504754 0.162439 11.00000 -1.50000 H20B 2 0.202367 0.464784 0.264622 11.00000 -1.50000 H20C 2 0.129748 0.477251 0.192240 11.00000 -1.50000 AFIX 0 C21 1 0.136382 0.171637 0.200244 11.00000 0.03147 0.03907 = 0.03598 -0.00635 0.00616 -0.00500 AFIX 137 H21A 2 0.102233 0.191334 0.251819 11.00000 -1.50000 H21B 2 0.175485 0.134338 0.226481 11.00000 -1.50000 H21C 2 0.103720 0.144414 0.152351 11.00000 -1.50000 AFIX 0 O1 3 0.078624 0.083671 -0.003906 11.00000 0.02711 0.03089 = 0.06531 -0.00299 -0.00291 -0.00136 AFIX 147 H1 2 0.029236 0.090206 0.000600 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 2005src1567 in I-4 C 0.770 H 0.320 O 0.660 C1 - C2 C2 - C1 C3 C3 - C2 C10 C4 C4 - C13 C5 C3 C5 - C6 C4 C6 - O1 C5 C7_a C27_b C7_a - C8_a C6 C8_a - C7_a C9_a C9_a - C8_a C27_b - C28_b C6 C28_b - C27_b C29_b C29_b - C28_b C10 - C12 C11 C3 C11 - C10 C12 - C10 C13 - C18 C14 C4 C14 - C15 C13 C19 C15 - C16 C14 C16 - C15 C17 C20 C17 - C16 C18 C18 - C17 C13 C21 C19 - C14 C20 - C16 C21 - C18 O1 - C6 Operators for generating equivalent atoms: $1 -y, x, -z 16313 Reflections read, of which 34 rejected -21 =< h =< 21, -21 =< k =< 13, -17 =< l =< 18, Max. 2-theta = 54.92 0 Systematic absence violations 0 Inconsistent equivalents 2349 Unique reflections, of which 0 suppressed R(int) = 0.0538 R(sigma) = 0.0373 Friedel opposites merged Maximum memory for data reduction = 3219 / 30749 Default effective X-H distances for T = -153.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 3979 / 290343 wR2 = 0.1091 before cycle 1 for 2349 data and 235 / 235 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 0.0902 0.0200 SAME/SADI C6 C7_a C6 C27_b Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 4. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.026 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.046 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.073; Restrained GooF = 1.076 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0460 * P )^2 + 1.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.62768 0.00148 -2.223 OSF 2 0.63786 0.00763 -0.085 FVAR 2 Mean shift/esd = 0.083 Maximum = -2.223 for OSF Max. shift = 0.007 A for H29C_b Max. dU = 0.000 for C9_a Least-squares cycle 2 Maximum vector length = 511 Memory required = 3979 / 290343 wR2 = 0.1088 before cycle 2 for 2349 data and 235 / 235 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint 0.0897 0.0200 SAME/SADI C6 C7_a C6 C27_b Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 4. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.026 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.046 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.070; Restrained GooF = 1.073 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0460 * P )^2 + 1.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.62700 0.00148 -0.462 OSF 2 0.63752 0.00761 -0.046 FVAR 2 Mean shift/esd = 0.029 Maximum = -0.462 for OSF Max. shift = 0.002 A for H29C_b Max. dU = 0.000 for C9_a Least-squares cycle 3 Maximum vector length = 511 Memory required = 3979 / 290343 wR2 = 0.1088 before cycle 3 for 2349 data and 235 / 235 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint 0.0896 0.0200 SAME/SADI C6 C7_a C6 C27_b Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 4. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.026 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.046 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.070; Restrained GooF = 1.073 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0460 * P )^2 + 1.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.62697 0.00147 -0.018 OSF 2 0.63743 0.00761 -0.011 FVAR 2 Mean shift/esd = 0.003 Maximum = -0.018 for OSF Max. shift = 0.000 A for H1 Max. dU = 0.000 for C28_b Least-squares cycle 4 Maximum vector length = 511 Memory required = 3979 / 290343 wR2 = 0.1088 before cycle 4 for 2349 data and 235 / 235 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint 0.0896 0.0200 SAME/SADI C6 C7_a C6 C27_b Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 4. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.026 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.046 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.070; Restrained GooF = 1.073 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0460 * P )^2 + 1.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.62697 0.00147 -0.001 OSF 2 0.63741 0.00761 -0.003 FVAR 2 Mean shift/esd = 0.001 Maximum = 0.006 for tors H19A Max. shift = 0.000 A for H19B Max. dU = 0.000 for C28_b Least-squares cycle 5 Maximum vector length = 511 Memory required = 3979 / 290343 wR2 = 0.1088 before cycle 5 for 2349 data and 235 / 235 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint 0.0896 0.0200 SAME/SADI C6 C7_a C6 C27_b Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 4. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.026 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.046 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.070; Restrained GooF = 1.073 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0460 * P )^2 + 1.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.62697 0.00147 0.000 OSF 2 0.63741 0.00761 -0.001 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.002 for tors H19A Max. shift = 0.000 A for H19B Max. dU = 0.000 for C28_b Least-squares cycle 6 Maximum vector length = 511 Memory required = 3979 / 290343 wR2 = 0.1088 before cycle 6 for 2349 data and 235 / 235 parameters Disagreeable restraints before cycle 6 Observed Target Error Sigma Restraint 0.0896 0.0200 SAME/SADI C6 C7_a C6 C27_b Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 4. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.026 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.046 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.070; Restrained GooF = 1.073 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0460 * P )^2 + 1.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.62697 0.00147 0.000 OSF 2 0.63740 0.00761 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.001 for tors H19A Max. shift = 0.000 A for H19B Max. dU = 0.000 for C28_b Least-squares cycle 7 Maximum vector length = 511 Memory required = 3979 / 290343 wR2 = 0.1088 before cycle 7 for 2349 data and 235 / 235 parameters Disagreeable restraints before cycle 7 Observed Target Error Sigma Restraint 0.0896 0.0200 SAME/SADI C6 C7_a C6 C27_b Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 4. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.026 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.046 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.070; Restrained GooF = 1.073 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0460 * P )^2 + 1.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.62697 0.00147 0.000 OSF 2 0.63740 0.00761 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for tors H20A Max. shift = 0.000 A for H20A Max. dU = 0.000 for C29_b Least-squares cycle 8 Maximum vector length = 511 Memory required = 3979 / 290343 wR2 = 0.1088 before cycle 8 for 2349 data and 235 / 235 parameters Disagreeable restraints before cycle 8 Observed Target Error Sigma Restraint 0.0896 0.0200 SAME/SADI C6 C7_a C6 C27_b Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 4. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.026 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.046 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.070; Restrained GooF = 1.073 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0460 * P )^2 + 1.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.62697 0.00147 0.000 OSF 2 0.63740 0.00761 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for tors H20A Max. shift = 0.000 A for H20C Max. dU = 0.000 for C28_b Largest correlation matrix elements 0.787 U12 C29_b / x C9_a -0.661 z C29_b / U23 C9_a -0.540 U23 C29_b / z C29_b -0.784 x C29_b / U12 C9_a 0.652 U23 C29_b / z C9_a 0.530 U23 C9_a / z C9_a -0.741 x C29_b / x C9_a 0.581 U23 C29_b / U23 C9_a -0.528 y C27_b / U22 C7_a 0.716 U12 C29_b / U12 C9_a -0.577 z C29_b / z C9_a 0.501 y C27_b / y C7_a 0.683 U12 C9_a / x C9_a 0.546 U22 C29_b / U22 C9_a -0.681 U12 C29_b / x C29_b 0.541 U22 C27_b / y C7_a Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.4054 0.0151 -0.0861 93 0.950 0.000 C1 C2 C3 H1B 0.3737 -0.0669 -0.0345 93 0.950 0.000 C1 C2 C3 H2 0.3054 0.0037 0.0711 43 0.950 0.000 C2 C1 C3 H3 0.3531 0.1418 -0.0328 13 1.000 0.000 C3 C2 C10 C4 H4 0.2157 0.1107 0.0795 13 1.000 0.000 C4 C13 C5 C3 H5A 0.2247 0.1690 -0.1119 23 0.990 0.000 C5 C6 C4 H5B 0.2132 0.0775 -0.0844 23 0.990 0.000 C5 C6 C4 H6 0.1019 0.1951 -0.0300 13 1.000 0.000 C6 O1 C5 C7_a H7A 0.0189 0.1661 -0.1590 23 0.990 0.000 C7_a C8_a C6 H7B 0.1015 0.2034 -0.1937 23 0.990 0.000 C7_a C8_a C6 H8A 0.0693 0.0364 -0.1980 23 0.990 0.000 C8_a C7_a C9_a H8B 0.1475 0.0778 -0.2404 23 0.990 0.000 C8_a C7_a C9_a H9A -0.0093 0.0998 -0.3149 137 0.980 0.000 C9_a C8_a H9A_a H9B 0.0595 0.0497 -0.3662 137 0.980 0.000 C9_a C8_a H9A_a H9C 0.0676 0.1442 -0.3561 137 0.980 0.000 C9_a C8_a H9A_a H27A 0.0963 0.0534 -0.1737 23 0.990 0.000 C27_b C28_b C6 H27B 0.0140 0.0979 -0.1500 23 0.990 0.000 C27_b C28_b C6 H28A 0.1441 0.1677 -0.2534 23 0.990 0.000 C28_b C27_b C29_b H28B 0.0654 0.2160 -0.2249 23 0.990 0.000 C28_b C27_b C29_b H29A 0.0673 0.0810 -0.3510 137 0.980 0.000 C29_b C28_b H29A_b H29B 0.0531 0.1709 -0.3847 137 0.980 0.000 C29_b C28_b H29A_b H29C -0.0123 0.1267 -0.3207 137 0.980 0.000 C29_b C28_b H29A_b H10 0.3733 0.2124 0.1145 13 1.000 0.000 C10 C12 C11 C3 H11A 0.5043 0.1689 0.1350 137 0.980 0.000 C11 C10 H11A H11B 0.4831 0.1659 0.0236 137 0.980 0.000 C11 C10 H11A H11C 0.4843 0.0856 0.0851 137 0.980 0.000 C11 C10 H11A H12A 0.3762 0.0611 0.2059 137 0.980 0.000 C12 C10 H12A H12B 0.3084 0.1266 0.2219 137 0.980 0.000 C12 C10 H12A H12C 0.3976 0.1440 0.2559 137 0.980 0.000 C12 C10 H12A H15 0.2715 0.4198 0.0458 43 0.950 0.000 C15 C16 C14 H17 0.1361 0.3210 0.2494 43 0.950 0.000 C17 C16 C18 H19A 0.3258 0.3544 -0.0751 137 0.980 0.000 C19 C14 H19A H19B 0.2879 0.2713 -0.1072 137 0.980 0.000 C19 C14 H19A H19C 0.3649 0.2727 -0.0400 137 0.980 0.000 C19 C14 H19A H20A 0.2175 0.5047 0.1625 137 0.980 0.000 C20 C16 H20A H20B 0.2023 0.4648 0.2646 137 0.980 0.000 C20 C16 H20A H20C 0.1298 0.4773 0.1921 137 0.980 0.000 C20 C16 H20A H21A 0.1023 0.1913 0.2519 137 0.980 0.000 C21 C18 H21A H21B 0.1755 0.1343 0.2264 137 0.980 0.000 C21 C18 H21A H21C 0.1037 0.1444 0.1524 137 0.980 0.000 C21 C18 H21A H1 0.0293 0.0904 0.0009 147 0.840 0.000 O1 C6 H1 2005src1567 in I-4 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.37504 -0.01049 -0.03784 1.00000 0.06397 0.05785 0.07470 -0.02866 -0.02713 0.03047 0.06551 0.00572 0.00020 0.00021 0.00028 0.00000 0.00201 0.00183 0.00225 0.00177 0.00183 0.00157 0.00099 H1A 0.40541 0.01512 -0.08611 1.00000 0.07861 0.00000 0.00000 H1B 0.37374 -0.06691 -0.03449 1.00000 0.07861 0.00000 0.00000 C2 0.33486 0.03209 0.02424 1.00000 0.03576 0.03533 0.05574 -0.01164 -0.01154 0.00700 0.04228 0.00445 0.00015 0.00015 0.00022 0.00000 0.00129 0.00128 0.00169 0.00127 0.00129 0.00100 0.00063 H2 0.30544 0.00368 0.07107 1.00000 0.05073 0.00000 0.00000 C3 0.33078 0.12114 0.02856 1.00000 0.02758 0.03291 0.03053 -0.00174 0.00103 0.00281 0.03034 0.00397 0.00013 0.00013 0.00017 0.00000 0.00107 0.00117 0.00115 0.00100 0.00097 0.00087 0.00049 H3 0.35310 0.14185 -0.03281 1.00000 0.03641 0.00000 0.00000 C4 0.24190 0.14778 0.03329 1.00000 0.02484 0.02894 0.02919 -0.00044 0.00196 0.00232 0.02766 0.00389 0.00013 0.00013 0.00017 0.00000 0.00103 0.00110 0.00114 0.00094 0.00093 0.00085 0.00047 H4 0.21566 0.11073 0.07945 1.00000 0.03319 0.00000 0.00000 C5 0.20116 0.13260 -0.06401 1.00000 0.03139 0.04369 0.03270 -0.00590 -0.00025 0.00528 0.03593 0.00428 0.00014 0.00016 0.00018 0.00000 0.00119 0.00137 0.00124 0.00112 0.00104 0.00102 0.00056 H5A 0.22466 0.16899 -0.11191 1.00000 0.04311 0.00000 0.00000 H5B 0.21322 0.07752 -0.08440 1.00000 0.04311 0.00000 0.00000 C6 0.11140 0.14376 -0.06432 1.00000 0.02997 0.05204 0.03340 -0.00297 -0.00272 0.00445 0.03847 0.00456 0.00014 0.00017 0.00019 0.00000 0.00120 0.00151 0.00133 0.00120 0.00104 0.00109 0.00059 H6_a 0.10187 0.19506 -0.03002 1.00000 0.04616 0.00000 0.00000 C7_a 0.07674 0.15583 -0.16448 0.63740 0.03361 0.03189 0.03660 0.00333 -0.00550 -0.00387 0.03403 0.00738 0.00024 0.00029 0.00031 0.00761 0.00210 0.00255 0.00267 0.00198 0.00176 0.00167 0.00114 H7A_a 0.01893 0.16607 -0.15897 0.63740 0.04084 0.00761 0.00000 H7B_a 0.10153 0.20337 -0.19373 0.63740 0.04084 0.00761 0.00000 C8_a 0.08975 0.08497 -0.22957 0.63740 0.03640 0.04577 0.04196 -0.00619 -0.00310 -0.00032 0.04138 0.00733 0.00025 0.00026 0.00032 0.00761 0.00222 0.00260 0.00274 0.00209 0.00189 0.00174 0.00126 H8A_a 0.06932 0.03640 -0.19800 0.63740 0.04965 0.00761 0.00000 H8B_a 0.14749 0.07777 -0.24044 0.63740 0.04965 0.00761 0.00000 C9_a 0.04816 0.09562 -0.32517 0.63740 0.04688 0.06447 0.04475 -0.00919 -0.00467 -0.00634 0.05203 0.01213 0.00051 0.00046 0.00051 0.00761 0.00300 0.00440 0.00349 0.00346 0.00249 0.00383 0.00178 H9A_a -0.00935 0.09979 -0.31491 0.63740 0.07805 0.00761 0.00000 H9B_a 0.05945 0.04973 -0.36616 0.63740 0.07805 0.00761 0.00000 H9C_a 0.06756 0.14419 -0.35607 0.63740 0.07805 0.00761 0.00000 C27_b 0.07183 0.10571 -0.15955 0.36260 0.03199 0.03045 0.03813 0.00491 -0.00051 -0.00350 0.03352 0.01285 0.00040 0.00050 0.00051 0.00761 0.00364 0.00431 0.00449 0.00353 0.00309 0.00288 0.00202 H27A_b 0.09628 0.05345 -0.17367 0.36260 0.04022 0.00761 0.00000 H27B_b 0.01403 0.09785 -0.14995 0.36260 0.04022 0.00761 0.00000 C28_b 0.08623 0.16278 -0.24171 0.36260 0.04424 0.03895 0.03850 -0.00346 -0.00449 -0.00656 0.04056 0.01222 0.00046 0.00043 0.00055 0.00761 0.00426 0.00416 0.00497 0.00332 0.00338 0.00300 0.00227 H28A_b 0.14409 0.16774 -0.25339 0.36260 0.04868 0.00761 0.00000 H28B_b 0.06538 0.21604 -0.22489 0.36260 0.04868 0.00761 0.00000 C29_b 0.04485 0.13260 -0.33279 0.36260 0.05395 0.05839 0.02886 -0.00057 -0.01130 -0.01140 0.04707 0.01825 0.00090 0.00073 0.00080 0.00761 0.00579 0.00709 0.00451 0.00524 0.00398 0.00659 0.00296 H29A_b 0.06733 0.08100 -0.35101 0.36260 0.07060 0.00761 0.00000 H29B_b 0.05312 0.17085 -0.38467 0.36260 0.07060 0.00761 0.00000 H29C_b -0.01225 0.12670 -0.32069 0.36260 0.07060 0.00761 0.00000 C10 0.38338 0.15388 0.11014 1.00000 0.03108 0.02824 0.03514 -0.00031 -0.00371 0.00175 0.03149 0.00403 0.00014 0.00013 0.00018 0.00000 0.00116 0.00111 0.00123 0.00101 0.00102 0.00089 0.00051 H10 0.37333 0.21239 0.11454 1.00000 0.03779 0.00000 0.00000 C11 0.47175 0.14254 0.08629 1.00000 0.02927 0.06126 0.04369 0.00274 -0.00346 -0.00298 0.04474 0.00487 0.00015 0.00018 0.00021 0.00000 0.00126 0.00170 0.00153 0.00135 0.00119 0.00116 0.00066 H11A 0.50431 0.16891 0.13498 1.00000 0.06711 0.00000 0.00000 H11B 0.48308 0.16585 0.02357 1.00000 0.06711 0.00000 0.00000 H11C 0.48429 0.08563 0.08510 1.00000 0.06711 0.00000 0.00000 C12 0.36475 0.11824 0.20700 1.00000 0.03908 0.05628 0.03674 0.00533 -0.00225 0.00328 0.04403 0.00500 0.00016 0.00018 0.00020 0.00000 0.00140 0.00165 0.00141 0.00132 0.00117 0.00118 0.00064 H12A 0.37620 0.06110 0.20592 1.00000 0.06605 0.00000 0.00000 H12B 0.30841 0.12657 0.22187 1.00000 0.06605 0.00000 0.00000 H12C 0.39760 0.14399 0.25588 1.00000 0.06605 0.00000 0.00000 C13 0.22776 0.23153 0.07283 1.00000 0.02382 0.03236 0.02733 -0.00019 -0.00183 0.00306 0.02784 0.00378 0.00013 0.00013 0.00016 0.00000 0.00104 0.00115 0.00109 0.00095 0.00092 0.00085 0.00046 C14 0.26179 0.30031 0.03233 1.00000 0.03070 0.03578 0.03408 0.00568 0.00235 0.00464 0.03352 0.00433 0.00014 0.00014 0.00018 0.00000 0.00114 0.00123 0.00120 0.00107 0.00105 0.00093 0.00052 C15 0.24813 0.37403 0.07399 1.00000 0.03165 0.02796 0.04149 0.00735 -0.00123 0.00052 0.03370 0.00422 0.00014 0.00014 0.00018 0.00000 0.00117 0.00114 0.00139 0.00107 0.00108 0.00092 0.00053 H15 0.27155 0.41977 0.04575 1.00000 0.04044 0.00000 0.00000 C16 0.20196 0.38362 0.15473 1.00000 0.03132 0.03010 0.03747 -0.00492 -0.01173 0.00363 0.03297 0.00398 0.00013 0.00014 0.00019 0.00000 0.00114 0.00117 0.00124 0.00105 0.00107 0.00090 0.00053 C17 0.16805 0.31603 0.19371 1.00000 0.02396 0.03606 0.02831 -0.00525 -0.00266 0.00259 0.02944 0.00385 0.00013 0.00013 0.00018 0.00000 0.00103 0.00117 0.00111 0.00101 0.00094 0.00087 0.00048 H17 0.13612 0.32105 0.24938 1.00000 0.03533 0.00000 0.00000 C18 0.17917 0.24086 0.15405 1.00000 0.02265 0.03169 0.02884 -0.00249 -0.00406 0.00021 0.02772 0.00368 0.00012 0.00013 0.00017 0.00000 0.00099 0.00114 0.00110 0.00095 0.00095 0.00085 0.00047 C19 0.31476 0.29959 -0.05521 1.00000 0.05837 0.03932 0.04805 0.01353 0.01835 0.00564 0.04858 0.00577 0.00018 0.00017 0.00021 0.00000 0.00174 0.00143 0.00168 0.00128 0.00138 0.00125 0.00071 H19A 0.32578 0.35438 -0.07508 1.00000 0.07287 0.00000 0.00000 H19B 0.28788 0.27126 -0.10720 1.00000 0.07287 0.00000 0.00000 H19C 0.36487 0.27266 -0.03998 1.00000 0.07287 0.00000 0.00000 C20 0.18654 0.46473 0.19723 1.00000 0.04972 0.03357 0.05399 -0.00890 -0.00947 0.00396 0.04576 0.00479 0.00017 0.00015 0.00023 0.00000 0.00156 0.00133 0.00163 0.00132 0.00138 0.00110 0.00067 H20A 0.21753 0.50474 0.16251 1.00000 0.06864 0.00000 0.00000 H20B 0.20229 0.46476 0.26465 1.00000 0.06864 0.00000 0.00000 H20C 0.12978 0.47731 0.19212 1.00000 0.06864 0.00000 0.00000 C21 0.13638 0.17162 0.20024 1.00000 0.03114 0.03871 0.03569 -0.00633 0.00617 -0.00502 0.03518 0.00429 0.00014 0.00014 0.00019 0.00000 0.00121 0.00128 0.00129 0.00111 0.00106 0.00096 0.00054 H21A 0.10228 0.19130 0.25186 1.00000 0.05277 0.00000 0.00000 H21B 0.17549 0.13429 0.22641 1.00000 0.05277 0.00000 0.00000 H21C 0.10368 0.14443 0.15236 1.00000 0.05277 0.00000 0.00000 O1 0.07863 0.08367 -0.00390 1.00000 0.02683 0.03053 0.06481 -0.00298 -0.00286 -0.00132 0.04072 0.00313 0.00010 0.00010 0.00015 0.00000 0.00082 0.00084 0.00125 0.00086 0.00086 0.00066 0.00045 H1 0.02929 0.09042 0.00095 1.00000 0.06109 0.00000 0.00000 Final Structure Factor Calculation for 2005src1567 in I-4 Total number of l.s. parameters = 235 Maximum vector length = 511 Memory required = 3746 / 24024 wR2 = 0.1088 before cycle 9 for 2349 data and 2 / 235 parameters Disagreeable restraints before cycle 9 Observed Target Error Sigma Restraint 0.0896 0.0200 SAME/SADI C6 C7_a C6 C27_b Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 4. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.026 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.046 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.070; Restrained GooF = 1.073 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0460 * P )^2 + 1.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0460 for 2036 Fo > 4sig(Fo) and 0.0570 for all 2349 data wR2 = 0.1088, GooF = S = 1.070, Restrained GooF = 1.073 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 22.00 for non-hydrogen and 34.00 for hydrogen atoms Principal mean square atomic displacements U 0.1234 0.0433 0.0298 C1 0.0668 0.0315 0.0285 C2 0.0345 0.0307 0.0258 C3 0.0303 0.0295 0.0231 C4 0.0478 0.0318 0.0282 C5 0.0535 0.0337 0.0282 C6 0.0431 0.0305 0.0286 C7_a 0.0505 0.0395 0.0341 C8_a 0.0689 0.0506 0.0366 C9_a 0.0410 0.0331 0.0264 C27_b 0.0490 0.0419 0.0307 C28_b 0.0690 0.0483 0.0238 C29_b 0.0375 0.0299 0.0271 C10 0.0621 0.0439 0.0283 C11 0.0580 0.0404 0.0336 C12 0.0334 0.0278 0.0223 C13 0.0428 0.0301 0.0277 C14 0.0448 0.0317 0.0246 C15 0.0486 0.0281 0.0223 C16 0.0395 0.0261 0.0227 C17 0.0337 0.0289 0.0206 C18 0.0767 0.0415 0.0275 C19 0.0645 0.0426 0.0302 C20 0.0474 0.0313 0.0268 C21 0.0653 0.0308 0.0261 O1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.031 0.047 0.061 0.076 0.093 0.112 0.142 0.182 0.269 1.000 Number in group 242. 243. 221. 238. 231. 239. 234. 230. 234. 237. GooF 1.292 1.034 0.979 1.079 1.009 1.042 1.148 1.030 0.994 1.043 K 1.963 1.096 1.043 1.055 1.028 1.014 1.023 0.998 1.000 0.997 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.33 1.67 inf Number in group 248. 228. 228. 249. 223. 240. 227. 239. 233. 234. GooF 0.982 1.058 0.988 0.947 0.891 1.009 1.070 1.150 1.200 1.332 K 0.997 1.093 1.043 1.056 1.015 1.021 0.980 0.981 1.000 1.004 R1 0.160 0.128 0.106 0.091 0.069 0.055 0.041 0.035 0.034 0.028 Recommended weighting scheme: WGHT 0.0450 1.7021 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) -6 9 3 68.20 4.02 6.13 0.016 1.47 6 6 6 450.29 191.99 5.84 0.108 1.51 10 10 0 141.48 13.45 5.83 0.028 1.19 3 12 3 744.14 352.53 5.75 0.146 1.31 0 12 0 458.93 89.94 5.64 0.074 1.40 -3 15 0 168.60 6.23 5.63 0.019 1.10 0 10 10 429.15 253.67 4.25 0.124 1.08 -3 12 3 60.24 16.84 4.14 0.032 1.31 9 9 0 197.97 92.95 4.05 0.075 1.32 0 6 0 1826.47 1370.23 3.96 0.288 2.80 7 7 0 368.33 259.59 3.58 0.125 1.70 6 10 14 158.31 56.29 3.39 0.058 0.82 -3 12 9 38.89 4.21 3.32 0.016 1.02 -6 8 0 347.37 256.02 3.30 0.124 1.68 1 20 3 408.27 278.03 3.24 0.130 0.83 3 3 6 2360.51 1948.38 3.17 0.343 2.01 -3 21 0 798.02 595.53 3.16 0.190 0.79 0 10 0 118.63 72.78 3.08 0.066 1.68 -4 5 5 286.04 215.11 3.04 0.114 1.92 0 0 12 45.92 12.68 3.01 0.028 1.17 0 12 12 118.72 61.42 2.89 0.061 0.90 4 16 4 55.52 22.91 2.88 0.037 0.98 -2 6 2 302.35 232.00 2.88 0.118 2.49 7 9 2 125.39 182.22 2.82 0.105 1.44 6 12 6 158.07 107.88 2.74 0.081 1.10 -5 7 0 2920.62 2520.36 2.67 0.390 1.95 7 13 0 116.78 174.14 2.64 0.103 1.14 11 15 6 156.13 95.81 2.63 0.076 0.84 -3 7 8 19.43 39.99 2.52 0.049 1.37 -3 9 0 135.81 90.24 2.51 0.074 1.77 -4 5 3 8.25 0.39 2.51 0.005 2.29 0 9 9 749.54 616.86 2.47 0.193 1.20 0 11 11 152.59 96.68 2.46 0.076 0.98 -6 20 0 49.36 1.98 2.44 0.011 0.81 0 1 3 4736.36 5392.29 2.42 0.571 4.50 -1 3 6 2252.44 1970.53 2.41 0.345 2.14 -2 4 12 111.32 161.60 2.41 0.099 1.11 3 19 6 723.95 590.03 2.37 0.189 0.82 -3 12 13 59.14 24.40 2.36 0.038 0.84 -7 16 7 42.08 5.63 2.35 0.018 0.87 -2 3 17 44.90 9.16 2.33 0.024 0.81 -3 17 10 71.97 30.51 2.33 0.043 0.80 -7 16 9 305.87 228.05 2.33 0.117 0.82 0 0 10 346.39 257.29 2.32 0.125 1.40 3 13 10 33.69 4.02 2.30 0.016 0.94 -7 18 5 51.79 0.86 2.30 0.007 0.83 -2 14 0 1156.79 1355.30 2.28 0.286 1.19 -11 12 11 58.73 17.07 2.27 0.032 0.80 -8 19 1 163.38 107.02 2.27 0.080 0.81 3 9 12 33.67 8.26 2.26 0.022 0.97 Bond lengths and angles C1 - Distance Angles C2 1.3131 (0.0042) H1A 0.9500 120.00 H1B 0.9500 120.00 120.00 C1 - C2 H1A C2 - Distance Angles C1 1.3131 (0.0042) C3 1.5000 (0.0033) 126.48 (0.32) H2 0.9500 116.76 116.76 C2 - C1 C3 C3 - Distance Angles C2 1.5000 (0.0033) C10 1.5456 (0.0033) 111.05 (0.19) C4 1.5615 (0.0029) 109.38 (0.19) 114.46 (0.19) H3 1.0000 107.20 107.20 107.20 C3 - C2 C10 C4 C4 - Distance Angles C13 1.5315 (0.0031) C5 1.5456 (0.0033) 113.66 (0.18) C3 1.5615 (0.0029) 115.32 (0.18) 109.84 (0.18) H4 1.0000 105.72 105.72 105.72 C4 - C13 C5 C3 C5 - Distance Angles C6 1.5209 (0.0033) C4 1.5456 (0.0033) 114.96 (0.20) H5A 0.9900 108.53 108.53 H5B 0.9900 108.53 108.53 107.53 C5 - C6 C4 H5A C6 - Distance Angles O1 1.4281 (0.0033) C5 1.5209 (0.0033) 107.09 (0.21) C7_a 1.5317 (0.0048) 119.26 (0.26) 113.36 (0.24) C27_b 1.6213 (0.0077) 92.82 (0.32) 111.15 (0.31) 31.10 (0.26) H6_a 1.0000 105.31 105.31 105.31 132.01 C6 - O1 C5 C7_a C27_b C7_a - Distance Angles C8_a 1.5157 (0.0060) C6 1.5317 (0.0048) 113.01 (0.34) H7A_a 0.9900 108.98 108.98 H7B_a 0.9900 108.98 108.98 107.77 C7_a - C8_a C6 H7A_a C8_a - Distance Angles C7_a 1.5157 (0.0060) C9_a 1.5204 (0.0077) 111.71 (0.42) H8A_a 0.9900 109.28 109.28 H8B_a 0.9900 109.28 109.28 107.94 C8_a - C7_a C9_a H8A_a C9_a - Distance Angles C8_a 1.5204 (0.0076) H9A_a 0.9800 109.47 H9B_a 0.9800 109.47 109.47 H9C_a 0.9800 109.47 109.47 109.47 C9_a - C8_a H9A_a H9B_a C27_b - Distance Angles C28_b 1.5171 (0.0096) C6 1.6213 (0.0077) 107.94 (0.56) H27A_b 0.9900 110.12 110.12 H27B_b 0.9900 110.12 110.12 108.44 C27_b - C28_b C6 H27A_b C28_b - Distance Angles C27_b 1.5171 (0.0096) C29_b 1.5384 (0.0110) 110.31 (0.65) H28A_b 0.9900 109.59 109.59 H28B_b 0.9900 109.59 109.59 108.13 C28_b - C27_b C29_b H28A_b C29_b - Distance Angles C28_b 1.5384 (0.0110) H29A_b 0.9800 109.47 H29B_b 0.9800 109.47 109.47 H29C_b 0.9800 109.47 109.47 109.47 C29_b - C28_b H29A_b H29B_b C10 - Distance Angles C12 1.5150 (0.0036) C11 1.5348 (0.0034) 110.22 (0.21) C3 1.5456 (0.0033) 113.69 (0.20) 110.43 (0.20) H10 1.0000 107.41 107.41 107.41 C10 - C12 C11 C3 C11 - Distance Angles C10 1.5348 (0.0034) H11A 0.9800 109.47 H11B 0.9800 109.47 109.47 H11C 0.9800 109.47 109.47 109.47 C11 - C10 H11A H11B C12 - Distance Angles C10 1.5150 (0.0036) H12A 0.9800 109.47 H12B 0.9800 109.47 109.47 H12C 0.9800 109.47 109.47 109.47 C12 - C10 H12A H12B C13 - Distance Angles C18 1.4087 (0.0031) C14 1.4092 (0.0032) 117.95 (0.20) C4 1.5315 (0.0031) 118.95 (0.19) 123.10 (0.20) C13 - C18 C14 C14 - Distance Angles C15 1.3890 (0.0033) C13 1.4092 (0.0032) 119.76 (0.22) C19 1.5147 (0.0037) 116.35 (0.22) 123.88 (0.22) C14 - C15 C13 C15 - Distance Angles C16 1.3805 (0.0035) C14 1.3890 (0.0033) 122.73 (0.22) H15 0.9500 118.63 118.63 C15 - C16 C14 C16 - Distance Angles C15 1.3805 (0.0035) C17 1.3835 (0.0034) 117.30 (0.21) C20 1.5103 (0.0034) 121.62 (0.24) 121.04 (0.24) C16 - C15 C17 C17 - Distance Angles C16 1.3835 (0.0034) C18 1.3930 (0.0031) 122.20 (0.22) H17 0.9500 118.90 118.90 C17 - C16 C18 C18 - Distance Angles C17 1.3930 (0.0031) C13 1.4087 (0.0031) 120.03 (0.21) C21 1.5135 (0.0032) 117.64 (0.21) 122.32 (0.20) C18 - C17 C13 C19 - Distance Angles C14 1.5147 (0.0037) H19A 0.9800 109.47 H19B 0.9800 109.47 109.47 H19C 0.9800 109.47 109.47 109.47 C19 - C14 H19A H19B C20 - Distance Angles C16 1.5103 (0.0034) H20A 0.9800 109.47 H20B 0.9800 109.47 109.47 H20C 0.9800 109.47 109.47 109.47 C20 - C16 H20A H20B C21 - Distance Angles C18 1.5135 (0.0032) H21A 0.9800 109.47 H21B 0.9800 109.47 109.47 H21C 0.9800 109.47 109.47 109.47 C21 - C18 H21A H21B O1 - Distance Angles C6 1.4281 (0.0033) H1 0.8400 109.47 O1 - C6 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.91 2.732(2) 165.9 O1-H1...O1_$1 FMAP and GRID set by program FMAP 2 3 18 GRID -1.667 -2 -1 1.667 2 1 R1 = 0.0570 for 2349 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.13 at 0.8676 0.1208 0.2003 [ 0.97 A from C28 ] Deepest hole -0.15 at 0.3036 0.2180 0.0061 [ 1.52 A from H19C ] Mean = 0.00, Rms deviation from mean = 0.03 e/A^3, Highest memory used = 3899 / 30621 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1208 0.1324 -0.2003 1.00000 0.05 0.13 0.97 C28 0.98 C7 1.03 H28A 1.04 C8 Q2 1 0.1707 0.2066 0.1857 1.00000 0.05 0.12 0.74 C18 0.85 C21 1.35 H21B 1.50 H21A Q3 1 0.3225 0.2548 -0.1028 1.00000 0.05 0.12 0.65 H19B 1.01 C19 1.17 H19C 1.72 H19A Q4 1 0.0963 0.0400 0.0189 1.00000 0.05 0.12 0.85 O1 1.20 H1 1.43 H1 2.02 O1 Q5 1 0.1849 0.2356 0.0997 1.00000 0.05 0.12 0.77 C18 0.82 C13 1.91 C17 1.94 C14 Shortest distances between peaks (including symmetry equivalents) 2 5 1.32 4 4 2.54 Time profile in seconds ----------------------- 0.09: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 1.67: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 2.30: Structure factors and derivatives 1.75: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.51: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.04: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.13: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2005src1567 finished at 13:47:59 Total CPU time: 6.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++